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DOE OSTI2025

Choline Chloride-Based Water-in-Salt Electrolyte for Efficient Iron Electrodeposition

Electrochemical production of iron is a promising low-cost and modular approach to replace the traditional blast furnace. Aqueous electrolytes for iron electrolysis are advantageous as they can be operated at near-ambient temperatures, but they suffer from inefficiencies due to the parasitic hydrogen evolution reaction. In this work, we identify a new water-in-salt electrolyte (WiSE) based on choline chloride (ChCl) for high coulombic efficiency (>85%) iron deposition. Electrochemical analysis of the partial current densities of iron plating and hydrogen co-evolution revealed that, at optimal WiSE compositions, water reduction is kinetically suppressed resulting in an increase in the Fe plating efficiency. Decreased coordination of water and increased coordination of choline’s alcohol group with the Fe 2+ ion were observed through 1 H NMR providing evidence that water reduction is kinetically suppressed in WiSE. Additionally, Raman spectroscopy revealed that complexation effects (with Cl – ) reduce Fe 2+ diffusion coefficients and corresponding limiting currents as the ChCl concentration is increased. This results in an optimal WiSE composition (4 M ChCl + 1 M FeCl 2 ) that provides kinetic suppression of HER but also low transport resistance to Fe plating yielding 85% coulombic efficiency at high current densities.

Sinclair, Nicholas Scott [Case Western Reserve Uni↗

NASA NTRS1991

The potential for crustal resources on Mars

Martian resources pose not only an interesting scientific challenge but also have immense astronautical significance because of their ability to enhance mission efficiency, lower launch and program costs, and stimulate the development of large Mars surface facilities. Although much terrestrial mineralization is associated with plate tectonics and Mars apparently possesses a thick, stationary lithosphere, the presence of crustal swells, rifting, volcanism, and abundant volatiles indicates that a number of sedimentary, hydrothermal, dry-magma mineral concentration processes may have operated on Mars. For example, in Colorado Plateau-style (roll-front) deposits, uranium precipitation is localized by redox variations in groundwater. Also, evaporites (either in salt pans or even interstitially in pore spaces) might concentrate Cl, Li, and K. Many Martian impact craters have been modified by volcanism and probably have been affected by rising magma bodies interacting with ground ice or water. Such conditions might produce hydrothermal circulations and element concentrations. If the high sulfur content found by the Viking landers typifies Martian abundances, sulfide ore bodies may have been formed locally. Mineral-rich Africa seems to share many volcanic and tectonic characteristics with portions of Mars and may suggest Mars' potential mineral wealth. For example, the rifts of Valles Marineris are similar to the rifts in east Africa, and may both result from a large mantle plume rising from the interior and disrupting the surface. The gigantic Bushveld complex of South Africa, an ancient layered igneous intrusion that contains ores of chromium and Pt-group metals, illustrates the sort of dry-magma processes that also could have formed local element concentrations on Mars, especially early in the planet's history when heat flow was higher.

Cordell, Bruce M.↗

NASA NTRS2007

Compositional Constraints on Hematite-Rich Spherule (Blueberry) Formation at Meridiani Planum, Mars

Meridiani Planum was chosen as the landing site for the Mars Exploration Rover Opportunity partially based on Mars Global Surveyor Thermal Emission Spectrometer data indicating an abundance of hematite. Hematite often forms through processes that involve water, so the site was a promising one to determine whether conditions on Mars were ever suitable for life. Opportunity struck pay dirt; it s Miniature Thermal Emission Spectrometer (Mini-TES) and Mossbauer Spectrometer (MB) confirmed the presence of hematite in sulfate-rich sedimentary beds and in lag deposits. Meridiani Planum rocks contain three main components: silicate phases, sulfate and possibly chloride salts, and ferric oxide phases such as hematite. Primary igneous phases are at low abundance despite the basaltic origin of the protoliths. Jarosite, an alkali ferric sulfate, was identified by Mossbauer. Some of the hematite is contained in the spherules, and some resides in finer grains in outcrops. Mossbauer and Mini-TES data indicate that hematite is a dominant constituent of the spherules. Panoramic Camera (Pancam) and Microscopic Imager (MI) images of spherule interiors show that hematite is present throughout. The exact composition of the spherules is unknown. Mini-TES only identifies a hematite signature in the spherules; any other constituents have an upper limit of 5-10% .The MB data are consistent with the spherules being composed of only hematite.

Schneider, A. L.↗

DOE OSTI2022

Atmospheric particle abundance and sea salt aerosol observations in the springtime Arctic: a focus on blowing snow and leads

Abstract. Sea salt aerosols play an important role in the radiation budget and atmospheric composition over the Arctic, where the climate is rapidly changing. Previous observational studies have shown that Arctic sea ice leads are an important source of sea salt aerosols, and modeling efforts have also proposed blowing snow sublimation as a source. In this study, size-resolved atmospheric particle number concentrations and chemical composition were measured at the Arctic coastal tundra site of Utqiaġvik, Alaska, during spring (3 April–7 May 2016). Blowing snow conditions were observed during 25 % of the 5-week study period and were overpredicted by a commonly used blowing snow parameterization based solely on wind speed and temperature. Throughout the study, open leads were present locally. During periods when blowing snow was observed, significant increases in the number concentrations of 0.01–0.06 µm particles (factor of 6, on average) and 0.06–0.3 µm particles (67 %, on average) and a significant decrease (82 %, on average) in 1–4 µm particles were observed compared to low wind speed periods. These size distribution changes were likely caused by the generation of ultrafine particles from leads and/or blowing snow, with scavenging of supermicron particles by blowing snow. At elevated wind speeds, both submicron and supermicron sodium and chloride mass concentrations were enhanced, consistent with wind-dependent local sea salt aerosol production. At moderate wind speeds below the threshold for blowing snow as well as during observed blowing snow, individual sea spray aerosol particles were measured. These individual salt particles were enriched in calcium relative to sodium in seawater due to the binding of this divalent cation with organic matter in the sea surface microlayer and subsequent enrichment during seawater bubble bursting. The chemical composition of the surface snowpack also showed contributions from sea spray aerosol deposition. Overall, these results show the contribution of sea spray aerosol production from leads on both aerosols and the surface snowpack. Therefore, if blowing snow sublimation contributed to the observed sea salt aerosol, the snow being sublimated would have been impacted by sea spray aerosol deposition rather than upward brine migration through the snowpack. Sea spray aerosol production from leads is expected to increase, with thinning and fracturing of sea ice in the rapidly warming Arctic.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1983

Monolithic lead salt-silicon focal plane development

This paper is a summary of work done in the development of monolithic lead salt-silicon infrared focal plane technology. The photoconductive detector materials, PbS and PbSe are chemically deposited onto premetallized silicon MOSFET integrated circuit wafers. A variety of structures based on an implanted PMOS process were fabricated and evaluated. Operational results of an eight-element PbS array multiplexed on-chip are presented along with radiometric measurements on other integrated PbS-silicon MOSFET structures. PbS imagery is shown using one element of a 20-element array integrated on-chip.

Barrett, J. R.↗

NASA NTRS1994

Metabolic activity of microorganisms in evaporites

Crystalline salt is generally considered so hostile to most forms of life that it has been used for centuries as a preservative. Here, we present evidence that prokaryotes inhabiting a natural evaporite crust of halite and gypsum are metabolically active while inside the evaporite for at least 10 months. In situ measurements demonstrated that some of these "endoevaporitic" microorganisms (probably the cyanobacterium Synechococcus Nageli) fixed carbon and nitrogen. Denitrification was not observed. Our results quantified the slow microbial activity that can occur in salt crystals. Implications of this study include the possibility that microorganisms found in ancient evaporite deposits may have been part of an evaporite community.

NASA Discipline Exobiology↗

DOE OSTI2026

Quantifying Outer- and Inner-Coordination Sphere Effects Using Uranium Redox Chemistry in Molten Salt Solutions

Defining the relative influence of intramolecular and intermolecular forces is a fundamental problem in chemistry that is difficult to quantify. To address this challenge, we developed a method to evaluate the relative impact of direct chemical bonding in the inner-coordination sphere vs effects from cations in the outer-coordination sphere by comparative analysis of uranium redox reactivity in various molten salts. We observed that outer-coordination sphere cations (M 1+ ) and inner-coordination sphere anions (X 1– ) both affected uranium redox reactivity, with more polarizing M 1+ and larger X 1– favoring uranium in low oxidation states. Changing M 1+ (Li, Na, K) shifted the U IV + e 1– ⇌ U III (U IV/III ) and U III + 3e 1– → U 0 metal potentials by +330 and +240 mV, respectively. Changing X 1– (Cl, Br, I) caused larger shifts of +440 mV for the U IV/III redox potential and +1060 mV for the U 0 metal deposition potential. Using Coulomb’s Law, we correlated these potentials with electrostatic interactions between UIII and the molten salt. This model provided a facile way of predicting redox chemistry within molten salts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1982

Correlation and prediction of thermophoretic and inertial effects on particle deposition from non-isothermal turbulent boundary layers

The problem of small particle deposition which can cause hot stage corrosion and/or fouling in combustion turbines operating on fuels containing ash or inorganic salts is investigated. Two boundary layer transport phenomena are shown to assume importance in these cases: particle thermophoresis (migration down a temperature gradient) and particle inertia. Thermophoretic and eddy transport across turbulent boundary layers without and with particle inertia effects are quantitatively analyzed. The effects of streamwise blade curvature on particle transport across turbulent boundary layers are determined. It is shown that these phenomena destroy the analogy between mass and heat transfer or mass and momentum transfer. Also studied are the effects on particle deposition of distributed or localized wall blowing, surface roughness, and mainstream turbulence.

Rosner, D. E.↗

NASA NTRS2021

Assessing Ceres’ Past and Current Habitability

Dwarf planet Ceres is a compelling target as an evolved ocean world with, at least, regional brine reservoirs and potentially ongoing geological activity. Situated in the Main Belt of asteroids, Ceres is the most water-rich body in the inner solar system (in relative abundance) and is accessible enough for a sample return with the resources of a typical medium-class (New Frontiers) NASA mission. NASA’s Dawn mission at Ceres revealed the presence of liquid, brine-driven activity, organic matter, and a rich salt chemistry. With this evidence, the overarching goals of the mission concept presented herein are to quantify Ceres’ current habitability potential and origin. A sample return from young evaporite deposits in Occator crater offers greater science return than an in situ exploration mission by enabling high-resolution analysis of (1) organic matter expected from terrestrial and chondritic analogs that are trapped in salt minerals and (2) isotopes of refractory elements for a similar cost and less science risk. The sample return concept would be executed with a single flight system due to Ceres’ relative proximity to Earth and low gravity. Solar electric propulsion was identified as the most cost-effective approach for getting to Ceres and back. De-orbiting, landing, and takeoff are performed with a throttleable monopropellant hydrazine system. The solar arrays are stowed prior to landing and takeoff. Sample acquisition builds on the pneumatic system designed by Honeybee Robotics. The sample return mission concept relies on the availability of key technologies: an enhanced landing vision system leveraging investments from Mars 2020; retractable/redeployable solar arrays, which have been demonstrated on the International Space Station but not at Ceres’ gravity; and an emerging design from upcoming missions for sample transfer from the pneumatic sampling system to the sample return capsule. Return of a sample of mass ~100 g from Ceres, maintained at ≤ -20°C, is without precedent for any currently advocated Ocean World mission, enabling a vast range of experimental techniques back on Earth with sensitivities and accuracies far beyond those feasible with in situ instruments. A sample of this size also enables analyses to benefit from techniques that will become available in the future.

Casillas, Raul Polit↗

NASA NTRS1987

Electrical properties of polyimides containing a near-surface deposit of silver

Films containing a surface or near-surface deposit of palladium, gold or copper metal as well as tin, cobalt, copper, or lithium oxides have been prepared by dissolving appropriate metal salts into poly(amide-acid)/N,N-dimethylacetamide solutions and curing the solvent cast films to temperatures up to 300 C. This preparation technique has been extended to evaluate the thermal, spectroscopic, and electrical characteristics of condensation polyimide films modified with silver nitrate. A near-surface deposit of metallic silver results but the reflective surface has high electrical resistivity (sheet resistivity) due to a polymer coating or overlayer above the metal. Details pertaining to the silver nitrate modified condensation polyimides are presented. Also, the applicability of the structural model and electrical model previously proposed for the cobalt oxide system are assessed.

Rancourt, J. D.↗

DOE OSTI2020

Fundamental Study of Uranium Dendrites Electrochemically Separated in Molten Salt with the Presence of Cerium

In this study, uranium was electrochemically separated in the presence of cerium in eutectic LiCl-KCl at varying concentrations of cerium and varying overpotentials. Harvested dendrites were then examined and analyzed for their morphological features and elemental composition using various analytical techniques. Conclusions: Increasing the applied overpotential causes the dendrites to evolve from relatively simple and large platelet-like crystals (25 mV), to a grid-like network with crystals having jagged and smooth features (50 mV, 100 mV), and finally into a very chaotic and complex crystal morphology (200 mV) for all uranium-cerium compositions explored. Varying the uranium:cerium concentration ratio did not have much effect on the uranium dendrite morphologies. EDS results show that cerium is not co-deposited on the surface of the dendrite crystals, ICP-MS results do show a presence of cerium in the volumetric composition. This is likely due to salt occlusion during the dendrite formation. XRD has been performed on several samples at the 25 mV overpotential with 1 wt% U and 0 wt% Ce in the molten salt eutectic. These results indicate that there is not salt occlusion within the dendrites during electrochemical separation. Additionally, the uranium metal quickly oxidizes during preparation for XRD.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2022

Concepts for the Future Exploration of Dwarf Planet Ceres’ Habitability

Dwarf planet Ceres is a compelling target for future exploration because it hosts at least regional brine reservoirs and potentially ongoing geological activity. As the most water-rich body in the inner solar system, it is a representative of a population of planetesimals that were likely a significant source of volatiles and organics to the inner solar system. Here we describe possible medium-class (around $1 billion) mission concepts that would determine both Ceres' origin and its current habitability potential. Habitability is addressed through a combination of geological, geophysical, and compositional investigations by (i) searching for evidence from orbit of past and ongoing geological activity near landforms interpreted as brine-driven volcanic structures and (ii) probing the brine distribution below one of these regions with electromagnetic sounding (in situ). Two approaches were considered for compositional measurements, which address both habitability and origins: (1) in situ exploration at two sites and (2) sample return from a single site. Both concepts targeted material at Occator crater, which is one of the youngest features on Ceres (∼20 Ma) and a site rich in evaporites evolved from recently erupted brine sourced from a region >35 km deep. We conclude that a sample return architecture from these young evaporite deposits offers greater science return by enabling high-resolution analysis of organic matter (trapped in salt minerals) and isotopes of refractory elements for a similar cost and less science risk than in situ analyses. This manuscript describes the six science objectives and the two implementation concepts considered to achieve those objectives.

Julie Castillo-Rogez↗

NASA NTRS2022

Concepts for the Future Exploration of Dwarf Planet Ceres' Habitability

Dwarf planet Ceres is a compelling target for future exploration because it hosts at least regional brine reservoirs and potentially ongoing geological activity. As the most water-rich body in the inner solar system, it is a representative of a population of planetesimals that were likely a significant source of volatiles and organics to the inner solar system. Here we describe possible medium-class (around $1 billion) mission concepts that would determine both Ceres’ origin and its current habitability potential. Habitability is addressed through a combination of geological, geophysical, and compositional investigations by (i) searching for evidence from orbit of past and ongoing geological activity near landforms interpreted as brine-driven volcanic structures and (ii) probing the brine distribution below one of these regions with electromagnetic sounding (in situ). Two approaches were considered for compositional measurements, which address both habitability and origins: (1) in situ exploration at two sites and (2) sample return from a single site. Both concepts targeted material at Occator crater, which is one of the youngest features on Ceres (∼20 Ma) and a site rich in evaporites evolved from recently erupted brine sourced from a region >35 km deep. We conclude that a sample return architecture from these young evaporite deposits offers greater science return by enabling high-resolution analysis of organic matter (trapped in salt minerals) and isotopes of refractory elements for a similar cost and less science risk than in situ analyses. This manuscript describes the six science objectives and the two implementation concepts considered to achieve those objectives.

Julie Castillo-Rogez↗

NASA NTRSDate not supplied

Sea Salt and Dust Optical Depths in the Caribbean and Equatorial Western Atlantic: A Multi-technique Analysis

Many instruments and algorithms can estimate aerosol optical depth (AOD) of the atmosphere. The Moderate Resolution Imaging Spectroradiometer (MODIS) onboard the Aqua spacecraft provides estimates at several wavelengths. The Synergized Optical Depth of Aerosols (SODA) algorithm utilizes the Cloud-Aerosol Lidar with Orthogonal Polarization (CALIOP) onboard the Cloud-Aerosol Lidar and Infrared Pathfinder Satellite Observation (CALIPSO) spacecraft and the Cloud Profiling Radar (CPR) onboard the CloudSat spacecraft’s ocean returns to estimate AOD. CALIOP routinely estimates AOD for all individual layers detected within a column and these can be summed to generate a total column approximation. With the release of the Version 4.51 Lidar Level 2 data products in October 2023, direct estimates of total column optical depth are now derived using the Ocean Derived Column Optical Depths (ODCOD) algorithm. In this poster we investigate the multispectral AOD estimates, and derived Angstrom exponents of marine sea salt and dust provided by MODIS, SODA, CALIOP, and ODCOD in a major dust transport and deposition region of the equatorial Atlantic Ocean.

optical depth↗

DOE OSTI2024

Intrinsic exchange bias from interfacial reconstruction in an epitaxial Ni x Co y Fe 3– x – y O 4 (111)/α-Al 2 O 3 (0001) thin film family

Intrinsic exchange bias is known as the unidirectional exchange anisotropy that emerges in a nominally single-component ferro-(ferri-)magnetic system. In this work, with magnetic and structural characterizations, we demonstrate that intrinsic exchange bias is a general phenomenon in (Ni, Co, Fe)-based spinel oxide films deposited on α-Al 2 O 3 (0001) substrates, due to the emergence of a rock-salt interfacial layer consisting of antiferromagnetic CoO from interfacial reconstruction. We show that in Ni x Co y Fe 3–x–y O 4 (111)/α-Al 2 O 3 (0001) films, intrinsic exchange bias and interfacial reconstruction have consistent dependences on Co concentration y, while the Ni and Fe concentration appears to be less important. This work establishes a family of intrinsic exchange bias materials with great tunability by stoichiometry and highlights the strategy of interface engineering in controlling material functionalities.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS1968

Preparation of silver-activated zinc sulfide thin films

Silver improves luminescence and reduces contamination of zinc sulfide phosphors. The silver is added after the zinc sulfide phosphors are deposited in thin films by vapor evaporation, but before calcining, by immersion in a solution of silver salt.

Feldman, C.↗

NASA NTRS2015

Evaluation of the Global Aerosol Microphysical ModelE2-TOMAS Model Against Satellite and Ground-Based Observations

The TwO-Moment Aerosol Sectional (TOMAS) microphysics model has been integrated into the state-of-the- art general circulation model, GISS ModelE2. This paper provides a detailed description of the ModelE2-TOMAS model and evaluates the model against various observations including aerosol precursor gas concentrations, aerosol mass and number concentrations, and aerosol optical depths. Additionally, global budgets in ModelE2-TOMAS are compared with those of other global aerosol models, and the ModelE2-TOMAS model is compared to the default aerosol model in ModelE2, which is a one-moment aerosol (OMA) model (i.e. no aerosol microphysics). Overall, the ModelE2- TOMAS predictions are within the range of other global aerosol model predictions, and the model has a reasonable agreement (mostly within a factor of 2) with observations of sulfur species and other aerosol components as well as aerosol optical depth. However, ModelE2-TOMAS (as well as ModelE2-OMA) cannot capture the observed vertical distribution of sulfur dioxide over the Pacific Ocean, possibly due to overly strong convective transport and over-predicted precipitation. The ModelE2-TOMAS model simulates observed aerosol number concentrations and cloud condensation nuclei concentrations roughly within a factor of 2. Anthropogenic aerosol burdens in ModelE2-OMA differ from ModelE2-TOMAS by a few percent to a factor of 2 regionally, mainly due to differences in aerosol processes including deposition, cloud processing, and emission parameterizations. We observed larger differences for naturally emitted aerosols such as sea salt and mineral dust, as those emission rates are quite different due to different upper size cutoff assumptions.

Lee, Y. H.↗

NASA NTRS2018

Thresholds of Detection and Identification of Halite Nodule Habitats in the Atacama Desert Using Remote Imaging

The guiding theme of Mars exploration is shifting from global and regional habitability assessment to biosignature detection. To locate features likely to contain biosignatures, it is useful to focus on the reliable identification of specific habitats with high biosignature preservation potential. Proposed chloride deposits on Mars may represent evaporitic environments conducive to the preservation of biosignatures. Analogous chloride- bearing, salt-encrusted playas (salars) are a habitat for life in the driest parts of the Atacama Desert, and are also environments with a taphonomic window. The specific geologic features that harbor and preserve microorganisms in Atacama salars are sub- meter to meter scale salt protuberances, or halite nodules. This study focuses on the ability to recognize and map halite nodules using images acquired from an unmanned aerial vehicle (UAV) at spatial resolutions ranging from mm/pixel to that of the highest resolution orbital images available for Mars.

Phillips, M. S.↗